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使用微波PECVD沉积介孔二氧化硅薄膜。

Deposition of Mesoporous Silicon Dioxide Films Using Microwave PECVD.

作者信息

Laux Marcel, Dreher Ralf, Emmerich Rudolf, Henning Frank

机构信息

Fraunhofer Institute for Chemical Technology, Joseph-von-Fraunhofer-Straße 7, 76327 Pfinztal, Germany.

Karlsruhe Institute of Technology, Institute of Vehicle System Technology, Rintheimer Querallee 2, 76131 Karlsruhe, Germany.

出版信息

Materials (Basel). 2025 Jul 7;18(13):3205. doi: 10.3390/ma18133205.

DOI:10.3390/ma18133205
PMID:40649693
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC12251488/
Abstract

Mesoporous silicon dioxide films have been shown to be well suited as adhesion-promoting interlayers for generating high-strength polymer-metal interfaces. These films can be fabricated via microwave plasma-enhanced chemical vapor deposition using the precursor hexamethyldisiloxane and oxygen as working gas. The resulting mesoporous structures enable polymer infiltration during overmolding, which leads to a nanoscale form-locking mechanism after solidification. This mechanism allows for efficient stress transfer across the interface and makes the resulting adhesion highly dependent on the morphology of the deposited film. To gain a deeper understanding of the underlying deposition mechanisms and improve process stability, this work investigates the growth behavior of mesoporous silica films using a multiple regression analysis approach. The seven process parameters coating time, distance, chamber pressure, substrate temperature, flow rate, plasma pulse duration, and pause-to-pulse ratio were systematically varied within a Design of Experiments framework. The resulting films were characterized by their free surface area, mean agglomerate diameter, and film thickness using digital image analysis, white light interferometry, and atomic force microscopy. The deposited films exhibit a wide range of morphological appearances, ranging from quasi-dense to dust-like structures. As part of this research, the free surface area varied from 15 to 55 percent, the mean agglomerate diameter from 17 to 126 nm, and the film thickness from 35 to 1600 nm. The derived growth model describes the deposition process with high statistical accuracy. Furthermore, all coatings were overmolded via injection molding and subjected to mechanical testing, allowing a direct correlation between film morphology and their performance as adhesion-promoting interlayers.

摘要

介孔二氧化硅薄膜已被证明非常适合作为促进粘附的中间层,用于生成高强度的聚合物-金属界面。这些薄膜可以通过微波等离子体增强化学气相沉积法制备,使用六甲基二硅氧烷前驱体和氧气作为工作气体。所得的介孔结构使得聚合物在包覆成型过程中能够渗透,从而在固化后形成纳米级的形状锁定机制。这种机制允许在界面上进行有效的应力传递,并使得所得的粘附力高度依赖于沉积薄膜的形态。为了更深入地了解潜在的沉积机制并提高工艺稳定性,本工作采用多元回归分析方法研究介孔二氧化硅薄膜的生长行为。在实验设计框架内,系统地改变了七个工艺参数:涂层时间、距离、腔室压力、基板温度、流速、等离子体脉冲持续时间和脉冲间歇比。使用数字图像分析、白光干涉测量法和原子力显微镜对所得薄膜的自由表面积、平均团聚体直径和薄膜厚度进行了表征。沉积的薄膜呈现出广泛的形态外观,从准致密结构到粉尘状结构不等。作为本研究的一部分,自由表面积从15%变化到55%,平均团聚体直径从17纳米变化到126纳米,薄膜厚度从35纳米变化到1600纳米。推导的生长模型以高统计精度描述了沉积过程。此外,所有涂层都通过注塑进行包覆成型并进行了机械测试,从而能够直接关联薄膜形态与其作为促进粘附中间层的性能。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/14e6/12251488/500e27eb401d/materials-18-03205-g019.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/14e6/12251488/eae7a2d2d0f6/materials-18-03205-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/14e6/12251488/6121edfcccba/materials-18-03205-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/14e6/12251488/35856a811957/materials-18-03205-g011.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/14e6/12251488/74470e8ad27a/materials-18-03205-g012.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/14e6/12251488/b8c4f5587068/materials-18-03205-g013.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/14e6/12251488/33b4e4488e1b/materials-18-03205-g014.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/14e6/12251488/e06b1d5dddb9/materials-18-03205-g015.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/14e6/12251488/967e1553c676/materials-18-03205-g016.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/14e6/12251488/a46ce3cc541b/materials-18-03205-g017.jpg
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